HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15432774, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 15432773 | HCID 15432773 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 15432774 | HCID 15432774 | — |
Reaction Steps
A solution that consists of 2 g of 17β-hydroxy-14α,15α-methylenestr-5-en-3-one in 95 ml of acetone and 5 ml of 5% aqueous hydrochloric acid is stirred for 2.5 hours at room temperature. Then, 10 ml of saturated aqueous sodium bicarbonate solution and 200 ml of water are added in succession. This solution is concentrated by evaporation in a vacuum rotary evaporator, whereby crystallization is used. The crystals are filtered off, dried, dissolved in acetone and applied to a silica gel column (0.063-0.2 mm, Merck). Chromatography with cyclohexane ethyl acetate 7:3 (v/v) as an eluant yields 17β-hydroxy-14α,15α-methylenestr-4-en-3-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06388109B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-f01d343ed274447688fd02f1b1407e76 |
| Source note | uspto-grants-2002_05 |